Benzoyl chloride → N'-t-butyl-N-cyclohexenylcarbonyl-N'-benzoylhydrazine

HRID 849763ノート

反応式

HRID 849763 の反応式
Cl.[C:2]([NH:6][NH2:7])([CH3:5])([CH3:4])[CH3:3].[OH-].[Na+].[C:10]1([C:16](Cl)=[O:17])[CH2:15][CH2:14][CH2:13][CH2:12][CH:11]=1.[C:19](Cl)(=[O:26])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>C1(C)C=CC=CC=1.CCCCCC>[C:2]([N:6]([C:19](=[O:26])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[NH:7][C:16]([C:10]1[CH2:15][CH2:14][CH2:13][CH2:12][CH:11]=1)=[O:17])([CH3:5])([CH3:4])[CH3:3]

参加物

7

反応物 4

HCID 7412Benzoyl chlorideHCID 14798Sodium Hydroxide3 回HCID 81889tert-Butylhydrazine monohydrochlorideHCID 1420661-Cyclohexenecarbonyl chloride

生成物 1

HCID 15451994N'-t-butyl-N-cyclohexenylcarbonyl-N'-benzoylhydrazine

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒2 回HCID 8058Hexane溶媒2 回

反応条件

温度
5 °C

実験手順

To a stirred suspension of t-butylhydrazine hydrochloride (0.86 g, 0.007M) in toluene (30 ml) was added 50% sodium hydroxide (0.55 g, 0.007M). After 15 minutes, the mixture was cooled to 5° C. and cyclohexenylcarbonyl chloride (1.0 g, 0.007M) and 50% sodium hydroxide (0.55 g, 0.007M) were added separately and simultaneously so as to maintain the reaction temperature below 10° C. After the addition, the reaction mixture was allowed to warm to room temperature and stirred for 1 hr. The mixture was diluted with hexane and the solid product isolated by filtration. This product (1.2 g, 0.006M) was dissolved in toluene (30 ml) and cooled on ice while stirring. To this mixture was added benzoylchloride (1.0 g, 0.007M) and 50% sodium hydroxide (1.3 g, 0.007M) simultaneously. After addition, the mixture was stirred for 1/2 hr., diluted with hexane and the solid product, N'-t-butyl-N-cyclohexenylcarbonyl-N'-benzoylhydrazine, isolated by filtration.

後処理

  1. temperaturesimultaneously so as to maintain the reaction temperature below 10° C
  2. additionAfter the addition
  3. temperatureto warm to room temperature
  4. customthe solid product isolated by filtration
  5. temperaturecooled on ice
  6. stirringwhile stirring
  7. additionAfter addition
  8. stirringthe mixture was stirred for 1/2 hr

出典と根拠

ORDレコード
ord-6d5ca1b9f4054febacf23bda7f174b4b
出典データセット
uspto-grants-2000_01
特許番号
US06013836

反応ノート

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